#------------------------------------------------------------------------------ #$Date: 2020-05-23 08:16:07 +0300 (Sat, 23 May 2020) $ #$Revision: 252320 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/34/2243406.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243406 loop_ _publ_author_name 'Khosa, Muhammad Kaleem' 'Wood, Paul T.' 'Humphrey, Simon M.' 'Harrison, William T. A.' _publ_section_title ; Hydrothermal synthesis and crystal structure of poly[bis(\m~3~-3,4-diaminobenzoato)manganese], a layered coordination polymer ; _journal_coeditor_code IS5538 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 909 _journal_page_last 913 _journal_paper_doi 10.1107/S2056989020006805 _journal_volume 76 _journal_year 2020 _chemical_formula_iupac '[Mn (C7 H7 N2 O2)2]' _chemical_formula_moiety 'C14 H14 Mn N4 O4' _chemical_formula_sum 'C14 H14 Mn N4 O4' _chemical_formula_weight 357.23 _chemical_name_systematic Poly[bis(\m~3~-3,4-diaminobenzoato-\k^3^N^3^,O,O')manganese(II)] _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 104.698(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.5171(5) _cell_length_b 4.4212(2) _cell_length_c 13.9752(7) _cell_measurement_reflns_used 5315 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 26.02 _cell_measurement_theta_min 1.02 _cell_volume 688.32(6) _computing_cell_refinement ; HKL Scalepack (Otwinowski & Minor, 1997) ; _computing_data_collection ; COLLECT (Nonius, 1998) ; _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997), SORTAV (Blessing, 1995) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and ATOMS (Shape Software, 2007) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2014/7 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5289 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.994 _diffrn_reflns_theta_min 2.053 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_T_max 0.983 _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SORTAV; Blessing, 1995) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.724 _exptl_crystal_description slab _exptl_crystal_F_000 366 _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.271 _refine_diff_density_min -0.275 _refine_ls_extinction_coef 0.012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018/3 (Sheldrick 2015) ; _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 119 _refine_ls_number_reflns 1345 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0310 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.5090P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.0742 _reflns_number_gt 1105 _reflns_number_total 1345 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file is5538sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2243406 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.805 _shelx_estimated_absorpt_t_max 0.952 _shelx_hkl_file ; -14 0 3 -0.11 2.79 -14 0 4 27.93 3.98 -14 0 5 2.15 3.44 -14 0 6 46.99 5.15 -14 0 7 6.64 4.18 -13 0 1 29.27 3.11 -13 0 2 -3.12 1.72 -13 0 3 61.09 6.69 -13 0 4 0.43 3.23 -13 0 5 217.82 15.55 -13 0 6 5.70 3.98 -13 0 7 46.66 5.05 -13 0 8 8.88 4.39 -13 0 9 188.30 14.33 -13 0 10 -0.32 4.68 13 1 -1 2.53 2.32 13 -1 -1 -0.33 2.60 13 1 -2 50.33 4.24 13 -1 -2 34.48 4.67 13 -1 -3 -0.32 3.25 13 1 -3 -0.74 1.91 13 -1 -4 61.98 5.31 13 1 -4 55.91 6.08 13 1 -5 -2.45 2.35 13 -1 -5 -3.12 2.80 13 1 -6 47.35 5.23 13 -1 -6 52.95 5.38 13 -1 -7 128.30 13.20 13 1 -7 114.58 11.52 13 1 -8 -3.09 3.83 13 -1 -8 6.94 4.49 13 -1 -9 79.98 6.73 13 1 -9 68.24 6.92 13 2 -2 -1.36 2.73 -13 2 2 -6.23 4.81 13 -2 -2 4.69 3.51 13 -2 -3 18.27 4.04 13 2 -3 18.32 3.58 -13 2 3 11.83 3.61 -13 2 4 19.76 3.73 13 2 -4 14.99 3.80 13 -2 -4 10.60 3.92 13 -2 -5 8.15 4.02 -13 2 5 1.98 3.19 13 2 -5 1.38 2.64 13 2 -6 -0.21 3.81 -13 2 6 -0.66 4.41 13 -2 -6 3.38 2.96 -12 0 1 -1.18 2.26 -12 0 2 11.12 2.70 12 0 -2 8.74 2.70 -12 0 3 -3.14 2.13 -12 0 4 57.99 4.55 -12 0 6 262.74 13.52 -12 0 7 -4.62 2.79 -12 0 8 347.67 21.27 -12 0 9 0.85 4.27 -12 0 10 80.28 9.59 -12 0 11 9.66 3.50 -12 0 12 16.42 5.08 12 -1 -1 125.77 8.98 -12 -1 1 122.37 7.47 12 1 -1 117.49 7.84 12 1 -2 31.10 3.19 12 -1 -2 28.26 3.81 12 -1 -2 35.99 4.29 12 -1 -3 27.75 3.01 12 -1 -3 31.12 4.13 12 1 -3 22.89 2.66 12 1 -4 15.36 2.56 12 -1 -4 7.57 3.79 12 -1 -4 17.47 3.22 12 1 -5 108.75 8.13 12 -1 -5 118.94 7.80 12 -1 -5 102.60 8.62 12 1 -6 3.84 3.52 12 -1 -6 0.64 2.68 12 -1 -6 -2.04 3.76 12 1 -7 11.30 2.88 12 -1 -7 20.80 3.33 12 1 -8 2.45 2.88 12 -1 -8 0.11 2.89 12 -1 -9 112.93 10.90 12 1 -9 102.39 8.52 12 -1 -10 -2.13 3.30 12 1 -10 3.61 3.08 12 1 -11 20.87 3.81 12 -1 -11 19.74 3.93 12 -1 -12 10.59 5.19 12 1 -12 8.99 3.70 12 -2 -1 24.92 3.31 12 2 -1 32.87 4.09 -12 2 1 33.63 4.14 12 2 -2 142.44 9.89 12 -2 -2 131.58 11.32 -12 2 2 142.72 10.50 -12 2 3 3.83 4.38 12 -2 -3 -2.33 2.55 12 2 -3 1.90 2.11 -12 2 4 58.45 6.15 12 2 -4 47.34 5.50 12 -2 -4 45.77 5.20 12 2 -5 56.54 6.25 -12 2 5 42.64 6.05 12 2 -6 81.20 9.13 -12 2 6 105.83 8.83 12 -2 -6 83.94 7.00 12 -2 -7 15.11 4.75 12 2 -7 15.70 3.29 12 2 -8 10.92 4.24 12 -2 -8 5.49 3.27 12 2 -9 16.64 3.50 12 -2 -9 15.09 3.69 12 2 -10 4.98 3.28 12 -2 -10 14.97 5.17 11 0 -1 47.85 4.00 -11 0 1 39.98 3.26 -11 0 2 2.13 2.47 11 0 -2 9.09 2.92 -11 0 3 1.90 2.69 11 0 -3 0.11 2.06 11 0 -3 5.94 2.59 11 0 -4 9.52 3.35 11 0 -4 -1.95 1.51 -11 0 4 1.34 2.12 11 0 -5 1447.52 65.97 11 0 -5 1368.41 67.51 11 0 -6 2.69 2.58 11 0 -6 -1.19 2.05 11 0 -7 5.05 3.01 11 0 -7 -0.54 1.73 -11 0 8 -2.78 4.18 -11 0 9 23.07 4.70 -11 0 10 0.43 3.09 -11 0 11 2.44 4.57 -11 0 12 -3.50 3.18 -11 0 13 87.72 8.16 -11 1 1 7.69 2.53 11 -1 -1 1.82 3.21 11 -1 -1 4.04 1.75 -11 -1 1 9.43 2.50 11 1 -1 3.81 2.22 -11 -1 1 4.87 2.21 11 -1 -2 68.21 5.68 -11 -1 2 67.88 4.55 -11 1 2 62.49 4.87 11 1 -2 80.34 5.54 -11 -1 3 0.23 2.03 11 -1 -3 4.12 2.82 11 1 -3 -1.70 2.02 11 -1 -3 0.43 2.04 -11 1 3 2.44 2.77 11 -1 -4 14.29 2.37 11 -1 -4 21.74 3.57 11 1 -4 18.46 2.56 -11 -1 4 6.51 3.48 11 -1 -5 15.64 2.91 11 1 -5 17.30 3.42 11 -1 -5 11.41 2.91 11 -1 -6 56.97 4.66 11 1 -6 51.45 3.85 11 -1 -6 47.87 4.74 11 -1 -7 69.84 7.63 11 -1 -7 62.93 4.58 11 1 -7 71.87 5.45 11 -1 -8 116.20 12.32 11 -1 -8 121.57 8.11 11 1 -8 106.39 8.43 11 1 -9 4.57 2.87 11 -1 -9 8.32 2.85 11 -1 -9 17.50 4.38 11 -1 -10 143.52 11.95 11 1 -10 128.11 11.17 11 1 -11 20.98 4.88 11 -1 -11 20.72 3.83 11 1 -12 70.78 6.78 11 -1 -12 77.50 8.07 -11 1 13 32.96 7.93 -11 -2 1 229.76 18.85 -11 2 1 327.60 17.87 -11 -2 1 306.28 22.06 11 2 -1 333.58 21.00 11 -2 -1 323.39 14.98 -11 2 2 16.23 3.38 -11 -2 2 17.37 2.67 -11 -2 2 4.58 4.24 11 -2 -2 11.44 3.50 11 2 -2 15.04 2.52 -11 2 3 147.66 9.64 11 -2 -3 144.79 10.01 11 2 -3 142.40 8.67 -11 2 4 5.37 3.50 11 -2 -4 3.17 3.70 11 2 -4 9.83 2.43 -11 2 5 13.06 4.06 11 2 -5 17.59 3.29 11 -2 -5 8.35 2.96 11 2 -6 -2.44 3.61 11 -2 -6 10.99 4.33 11 -2 -6 5.60 3.62 11 -2 -7 17.76 3.86 11 -2 -7 14.27 3.38 11 2 -7 22.18 4.14 11 2 -8 -1.70 2.76 11 -2 -8 0.32 2.96 11 -2 -9 98.75 7.95 11 2 -9 93.12 7.76 11 2 -10 8.58 4.45 11 -2 -10 2.74 5.07 11 2 -11 29.33 5.19 11 -2 -11 21.84 4.12 11 3 -1 13.00 2.50 11 -3 -1 24.17 4.22 -11 3 1 23.26 4.22 11 -3 -2 25.01 3.40 -11 3 2 36.11 4.34 11 3 -2 37.87 3.86 11 3 -3 -0.63 3.35 -11 3 3 1.52 4.57 11 -3 -3 0.31 3.91 11 -3 -4 12.17 3.30 -11 3 4 10.02 3.38 11 3 -4 9.56 2.84 11 -3 -5 2.79 3.10 -11 3 5 5.46 4.37 11 3 -5 4.53 2.84 11 3 -6 37.27 4.12 -11 3 6 39.82 4.06 11 -3 -6 41.73 5.40 11 3 -7 12.27 3.39 -11 3 7 13.59 4.06 11 -3 -7 13.49 4.36 -11 3 8 112.83 9.28 11 -3 -8 117.19 9.72 11 3 -8 125.90 11.15 -10 0 1 -0.67 1.90 10 0 -1 0.22 1.73 10 0 -2 265.01 12.92 -10 0 2 229.66 17.91 10 0 -2 281.21 12.23 -10 0 3 1.34 2.34 10 0 -3 0.11 7.78 10 0 -3 3.68 3.03 10 0 -4 13.52 2.27 -10 0 4 7.78 2.67 10 0 -4 11.36 2.49 10 0 -5 3.03 1.95 -10 0 5 0.55 1.89 10 0 -5 2.59 2.48 10 0 -6 17.18 2.06 10 0 -6 10.55 2.80 10 0 -7 -1.51 1.62 10 0 -7 1.50 2.69 10 0 -8 2.16 1.73 10 0 -8 0.32 4.18 10 0 -9 1.08 1.62 10 0 -9 -3.95 2.99 -10 0 10 19.82 3.62 -10 0 11 -0.32 3.19 -10 0 12 51.99 6.05 -10 0 13 -2.65 3.18 -10 0 14 55.24 7.09 -10 -1 1 241.75 10.53 10 -1 -1 218.50 12.52 -10 1 1 219.30 11.56 -10 -1 1 249.68 18.37 10 -1 -1 208.11 12.11 10 1 -1 224.73 10.74 -10 1 2 48.83 4.30 10 -1 -2 48.16 4.04 -10 -1 2 53.19 3.73 10 1 -2 54.56 3.94 -10 -1 2 46.09 3.55 10 -1 -2 59.93 4.32 10 -1 -3 0.32 2.90 -10 1 3 4.53 2.65 10 -1 -3 -3.79 2.82 -10 -1 3 -6.83 2.80 10 1 -3 -5.76 2.66 10 -1 -4 16.93 3.13 -10 -1 4 17.86 3.24 10 -1 -4 14.49 2.60 -10 1 4 13.73 2.33 10 1 -4 8.75 3.10 -10 -1 5 477.80 34.55 -10 1 5 448.91 31.01 10 -1 -5 492.24 36.35 10 -1 -5 520.43 27.21 10 1 -5 506.94 28.61 10 -1 -6 11.19 3.66 10 -1 -6 12.41 2.29 10 1 -6 13.98 2.67 10 -1 -7 126.61 7.08 10 -1 -7 116.40 7.75 10 1 -7 112.78 8.02 10 -1 -8 2.98 1.99 10 -1 -8 5.24 2.78 10 1 -8 5.86 2.66 10 -1 -9 194.34 12.33 10 1 -9 195.60 11.85 10 -1 -10 -0.43 3.09 10 1 -10 2.44 2.87 10 1 -11 39.22 3.93 10 -1 -11 35.41 4.36 10 1 -12 13.98 4.66 10 -1 -12 9.23 3.40 10 1 -13 44.64 6.03 10 -1 -13 42.28 6.36 10 -1 -14 29.73 5.40 10 1 -14 33.30 5.50 -10 -2 1 0.34 1.94 -10 -2 1 2.56 1.67 -10 2 1 4.99 2.06 10 -2 -1 -1.40 2.59 -10 2 1 2.49 2.82 10 -2 -1 1.48 2.32 10 2 -1 4.40 2.52 -10 2 2 167.48 10.57 10 2 -2 174.05 11.70 10 -2 -2 180.15 10.00 10 -2 -2 170.12 10.41 -10 -2 2 152.11 10.56 -10 -2 2 163.03 12.37 -10 -2 3 50.49 4.24 -10 2 3 62.68 4.70 10 -2 -3 49.79 3.95 -10 -2 3 39.59 4.11 10 2 -3 45.92 4.65 10 -2 -3 48.65 4.02 -10 2 4 169.89 10.10 10 2 -4 155.66 11.35 10 -2 -4 159.85 8.12 10 -2 -4 159.17 9.98 10 -2 -5 9.93 2.85 -10 2 5 11.95 2.85 10 2 -5 11.98 2.54 10 -2 -5 13.00 3.97 10 2 -6 17.51 2.97 10 -2 -6 15.32 3.17 10 -2 -6 24.72 4.22 10 -2 -7 4.35 2.68 10 2 -7 11.04 3.93 10 -2 -7 6.76 4.12 10 -2 -8 112.46 8.38 10 2 -8 131.40 10.96 10 -2 -9 15.54 3.49 10 2 -9 25.57 3.51 10 2 -10 108.15 8.41 10 -2 -10 120.05 10.70 10 -2 -11 13.63 3.70 10 2 -11 15.47 4.77 10 2 -12 55.80 7.53 10 -2 -12 61.13 7.30 10 2 -13 16.72 4.34 10 -2 -13 17.09 4.01 10 3 -1 -1.77 3.02 10 -3 -1 1.13 2.77 -10 3 1 -3.02 4.43 10 -3 -2 0.62 2.78 10 3 -2 0.42 2.30 -10 3 2 4.44 4.33 10 -3 -3 158.48 9.55 -10 3 3 155.11 10.47 10 3 -3 149.91 10.08 10 -3 -4 3.30 2.99 10 3 -4 7.25 2.73 -10 3 4 1.20 7.18 10 3 -5 37.42 4.12 10 -3 -5 31.54 4.66 -10 3 5 46.09 4.16 -10 3 6 13.97 4.26 10 -3 -6 16.38 3.84 10 3 -6 20.50 3.38 10 -3 -7 76.27 7.71 10 3 -7 68.47 6.89 -10 3 7 73.93 5.72 10 -3 -8 -5.94 4.69 -10 3 8 1.64 2.41 10 3 -8 7.63 4.45 10 -3 -9 18.05 5.22 -10 3 9 14.14 2.74 10 3 -9 13.46 3.50 10 3 -10 3.82 3.29 10 -3 -10 0.52 8.57 9 0 -1 182.35 7.49 9 0 -1 193.83 9.38 -9 0 1 166.96 10.06 9 0 -2 2.48 2.38 9 0 -2 -1.63 2.71 -9 0 2 -1.11 2.22 9 0 -3 22.87 2.60 9 0 -3 18.60 2.49 -9 0 3 13.98 2.00 9 0 -4 -2.38 1.95 -9 0 4 2.88 1.77 9 0 -4 1.41 2.70 9 0 -5 259.08 10.17 9 0 -5 270.18 12.28 -9 0 5 213.98 11.45 9 0 -6 0.65 2.58 9 0 -6 -0.86 1.73 -9 0 6 -0.22 1.98 9 0 -7 37.81 2.93 9 0 -7 43.16 4.62 -9 0 7 39.10 3.31 9 0 -8 3.58 1.84 9 0 -8 5.46 4.28 9 0 -9 4.49 1.86 9 0 -9 -3.10 2.99 -9 0 10 4.48 4.37 -9 0 11 61.16 4.80 -9 0 12 -2.76 3.19 -9 0 13 98.46 7.55 -9 0 14 2.23 4.56 -9 0 15 4.03 3.50 -9 -1 1 142.01 6.58 -9 1 1 147.82 7.69 9 1 -1 145.95 7.02 9 -1 -1 140.95 7.79 -9 -1 1 139.00 8.39 9 -1 -1 151.11 6.71 -9 -1 2 277.79 16.38 9 -1 -2 275.54 13.58 -9 -1 2 238.78 15.73 9 -1 -2 284.50 10.78 -9 1 2 290.41 13.04 9 1 -2 286.25 12.39 9 -1 -3 446.68 26.44 -9 1 3 446.06 23.48 -9 -1 3 411.87 21.13 9 1 -3 476.50 20.68 9 -1 -3 445.29 19.45 -9 1 4 341.57 17.55 9 1 -4 330.27 15.76 9 -1 -4 365.90 17.21 9 -1 -4 325.12 23.08 -9 -1 4 306.57 20.76 9 -1 -5 30.38 4.10 9 1 -5 38.94 3.10 9 -1 -5 33.32 2.85 -9 -1 5 31.98 3.33 -9 1 5 36.27 3.88 9 -1 -6 226.59 16.61 9 -1 -6 254.58 12.28 -9 -1 6 211.19 15.63 9 1 -6 236.84 11.06 -9 1 6 202.26 11.68 9 1 -7 7.88 4.16 9 -1 -7 7.72 2.79 9 -1 -8 71.18 5.79 9 1 -8 77.79 5.87 9 1 -9 3.19 3.72 9 -1 -9 -0.32 3.85 9 1 -10 96.08 7.35 9 -1 -10 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10.09 -9 -2 -5 157.04 10.11 9 -2 5 196.64 9.82 -9 2 -6 16.37 3.75 -9 -2 -6 18.06 3.61 -9 2 -7 45.06 4.61 -9 -2 -7 50.64 6.10 -9 2 -8 1.18 4.60 -9 -2 -8 6.48 2.23 9 3 0 143.82 8.84 -9 3 0 139.30 8.21 -9 -3 0 112.33 8.69 -9 -3 0 140.15 8.62 9 -3 0 159.17 9.41 9 3 1 46.41 3.63 -9 3 -1 51.11 5.38 -9 -3 -1 41.92 3.67 9 -3 1 51.92 4.94 -9 3 -2 6.97 4.72 9 -3 2 12.42 2.57 -9 3 -3 8.78 3.43 -9 -3 -3 2.07 2.39 9 -3 3 -0.93 2.98 -9 3 -4 41.18 4.92 9 -3 4 64.95 4.88 -9 3 -5 2.89 3.53 9 -3 5 6.29 2.79 9 3 6 17.09 4.17 -9 4 0 57.54 6.07 9 -4 0 56.14 5.41 -9 4 -1 118.34 11.57 9 -4 1 123.94 9.02 10 0 0 113.89 5.21 -10 0 0 97.28 5.71 -10 0 0 93.73 6.28 10 0 1 -1.07 1.61 -10 0 -1 -0.66 1.66 -10 0 -1 9.32 4.28 10 0 2 28.55 2.24 -10 0 -2 30.74 2.51 -10 0 -2 38.64 4.62 10 0 3 -1.58 0.85 -10 0 -3 5.83 4.51 -10 0 -4 12.46 4.30 -10 0 -4 -3.04 3.69 -10 0 -5 -4.09 4.64 -10 0 -5 -4.97 3.89 -10 0 -6 41.51 4.65 -10 0 -6 35.75 3.99 -10 0 -7 4.54 5.21 -10 0 -7 2.26 2.79 -10 0 -8 54.79 9.10 -10 0 -8 83.23 7.42 10 1 0 29.88 3.06 -10 1 0 27.79 2.18 -10 -1 0 28.58 2.39 -10 -1 0 28.27 3.54 10 -1 0 28.43 2.96 10 -1 0 26.90 3.43 10 1 1 31.96 2.63 -10 1 -1 33.75 2.92 -10 1 -1 35.90 4.57 -10 -1 -1 23.43 2.85 -10 -1 -1 24.14 3.66 10 -1 1 26.08 2.97 10 -1 1 30.62 3.00 10 1 2 42.44 2.73 -10 1 -2 45.00 2.80 -10 1 -2 37.18 3.80 -10 -1 -2 38.98 2.97 -10 -1 -2 38.66 4.45 10 -1 2 35.55 2.87 10 -1 2 37.64 3.33 10 1 3 235.27 11.48 -10 1 -3 212.38 17.34 -10 1 -3 228.26 11.27 -10 -1 -3 238.36 13.76 10 -1 3 223.46 23.87 -10 1 -4 20.90 5.14 -10 1 -4 23.81 3.99 -10 -1 -4 15.52 5.25 10 -1 4 14.94 1.97 -10 1 -5 53.70 5.93 -10 1 -5 66.90 5.60 -10 -1 -5 53.25 5.38 -10 1 -6 -6.70 3.62 -10 1 -6 10.42 4.51 -10 -1 -6 1.34 5.04 -10 -1 -6 0.32 3.45 -10 1 -7 24.08 5.94 -10 1 -7 45.31 4.41 -10 -1 -7 25.53 4.48 -10 -1 -7 36.29 4.30 -10 1 -8 4.72 4.62 -10 -1 -8 -5.49 4.14 -10 -1 -8 2.25 2.36 10 2 0 169.24 8.91 -10 2 0 141.80 9.53 -10 2 0 176.82 10.29 -10 -2 0 132.72 8.57 -10 -2 0 141.40 10.56 10 -2 0 164.43 8.44 10 2 1 2.19 2.08 -10 2 -1 1.29 1.72 -10 2 -1 -5.28 2.91 -10 -2 -1 1.27 2.30 -10 -2 -1 0.79 3.15 10 -2 1 -2.43 2.75 10 2 2 195.29 12.20 -10 -2 -2 145.17 15.36 10 2 3 1.46 1.56 -10 2 -3 5.59 4.62 -10 -2 -3 -4.52 3.73 10 -2 3 -0.11 2.23 -10 2 -4 214.53 13.76 -10 -2 -4 207.69 14.76 10 -2 4 215.95 15.96 -10 2 -5 3.22 3.32 -10 -2 -5 5.54 4.41 -10 2 -6 108.18 9.01 -10 -2 -6 97.56 8.28 -10 2 -7 3.85 3.53 -10 -2 -7 1.13 4.97 10 3 0 47.00 4.16 -10 3 0 41.17 4.64 -10 -3 0 45.84 4.22 10 -3 0 55.12 6.07 10 3 1 9.43 2.80 -10 3 -1 22.05 3.87 -10 -3 -1 10.38 3.20 10 -3 1 20.12 3.80 -10 3 -2 20.94 3.97 -10 -3 -2 15.76 2.86 10 -3 2 26.71 2.89 -10 3 -3 -1.82 5.04 -10 -3 -3 -0.23 3.65 10 -3 3 2.26 2.16 -10 3 -4 8.99 5.25 -10 -3 -4 7.99 4.11 10 -3 4 7.01 2.17 11 0 0 -1.29 1.83 -11 0 0 1.56 1.34 11 0 1 3.53 1.60 -11 0 -1 -0.88 2.86 11 0 2 0.64 1.17 -11 0 -2 1.65 4.07 11 0 3 73.33 6.08 -11 0 -4 -0.44 3.20 -11 0 -4 2.72 2.94 -11 0 -5 37.87 6.20 -11 0 -5 42.47 5.10 -11 0 -6 -12.09 5.21 -11 0 -6 -1.40 4.10 11 0 7 2.15 4.31 11 1 0 109.36 6.24 -11 1 0 96.66 7.00 -11 -1 0 88.32 8.47 -11 -1 0 94.47 7.55 11 -1 0 85.35 6.70 11 -1 0 100.03 7.64 11 1 1 55.78 3.37 -11 1 -1 53.12 4.91 -11 -1 -1 31.64 4.55 11 -1 1 48.24 4.07 11 1 2 132.00 9.13 -11 1 -2 129.88 8.60 -11 -1 -2 121.68 9.60 11 -1 2 139.58 7.74 -11 1 -3 14.95 3.36 -11 -1 -3 10.27 4.47 -11 1 -4 50.77 5.93 -11 1 -4 48.07 5.51 -11 -1 -4 74.85 6.39 -11 1 -5 -0.66 3.62 -11 1 -5 3.45 3.23 -11 -1 -5 2.80 3.59 -11 1 -6 62.42 6.35 -11 -1 -6 57.41 6.51 -11 -1 -6 57.69 5.21 11 2 0 6.58 2.40 -11 2 0 9.64 4.33 -11 -2 0 3.25 2.91 11 -2 0 0.43 3.08 11 2 1 88.01 5.32 -11 2 -1 91.53 7.03 -11 -2 -1 93.26 8.57 11 -2 1 88.14 6.23 -11 2 -2 -2.70 4.64 -11 -2 -2 -1.47 2.48 11 -2 2 0.11 1.60 -11 2 -3 116.02 7.98 -11 -2 -3 99.44 8.28 -11 2 -4 -2.79 3.22 -11 -2 -4 1.25 4.30 -11 2 -5 42.93 5.15 -11 -2 -5 47.58 5.11 11 3 0 18.16 3.11 -11 3 0 12.85 5.08 11 -3 0 11.01 3.81 -11 3 -1 -2.91 4.96 11 -3 1 4.74 3.40 12 0 0 62.17 5.58 12 0 1 1.17 1.60 -12 0 -1 -5.07 2.98 12 0 2 142.06 10.54 -12 0 -3 8.62 5.42 -12 0 -3 -0.55 3.07 -12 0 -4 43.64 6.10 -12 0 -4 55.56 5.69 -12 0 -5 5.99 3.99 -12 0 -5 -2.17 3.15 12 1 0 16.85 2.32 -12 1 0 18.11 3.62 -12 -1 0 12.99 4.00 12 -1 0 14.93 2.18 -12 1 -1 42.64 6.02 -12 -1 -1 48.06 4.24 12 -1 1 48.90 5.24 -12 1 -2 3.05 3.27 -12 -1 -2 -7.47 4.24 -12 1 -3 68.53 6.85 -12 -1 -3 76.16 6.73 -12 1 -4 -7.80 4.77 -12 -1 -4 -0.56 4.93 12 2 0 37.89 4.07 -12 2 0 47.33 4.56 12 -2 0 36.31 4.29 -12 2 -1 -2.17 4.87 12 -2 1 -3.86 2.68 -12 2 -2 10.37 5.19 -12 -2 -2 -1.13 3.73 -13 1 0 48.26 4.95 -13 -1 0 50.96 5.46 -13 1 -1 12.27 3.73 -13 -1 -1 -0.45 3.12 -13 -1 -1 -0.45 3.12 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 34362 _shelx_res_file ; TITL pw0710 in P2(1)/n pw0710t.res created by SHELXL-2018/3 at 18:27:25 on 19-Mar-2020 CELL 0.71073 11.5171 4.4212 13.9752 90 104.698 90 ZERR 2 0.0005 0.0002 0.0007 0 0.003 0 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O MN UNIT 28 28 8 8 2 L.S. 4 BOND $H conf FMAP 2 PLAN 10 ACTA htab eqiv $1 x,y-1,z mpla 3 c7 o1 o2 mn1 mn1_$1 mpla 6 c1 c2 c3 c4 c5 c6 n1 n2 c7 TEMP -93 SIZE 0.23 0.1 0.05 rem yellow(?) slab REM Instructions for potential hydrogen bonds EQIV $3 -x+1/2, y+1/2, -z+1/2 HTAB N1 O1_$3 EQIV $8 -x+3/2, y-1/2, -z+1/2 HTAB N2 N2_$8 EQIV $9 x+1/2, -y-1/2, z+1/2 HTAB N2 O2_$9 WGHT 0.028200 0.509000 EXTI 0.011512 FVAR 0.59725 MN1 5 0.000000 0.500000 0.000000 10.50000 0.01897 0.01729 = 0.01865 0.00021 0.00188 0.00075 C1 1 0.321859 -0.048844 0.117171 11.00000 0.01942 0.01878 = 0.01961 0.00233 0.00343 -0.00101 C2 1 0.364142 0.105477 0.205980 11.00000 0.01979 0.01765 = 0.02245 0.00213 0.00640 0.00215 AFIX 43 H2 2 0.312438 0.241153 0.228031 11.00000 -1.20000 AFIX 0 C3 1 0.480369 0.064241 0.262641 11.00000 0.01976 0.02002 = 0.01710 0.00132 0.00329 -0.00275 C4 1 0.557986 -0.133482 0.230631 11.00000 0.01652 0.02030 = 0.02380 0.00387 0.00406 -0.00147 C5 1 0.516339 -0.280230 0.139849 11.00000 0.02326 0.02761 = 0.02653 -0.00220 0.00878 0.00595 AFIX 43 H5 2 0.568982 -0.407707 0.115733 11.00000 -1.20000 AFIX 0 C6 1 0.399253 -0.241873 0.084702 11.00000 0.02579 0.02564 = 0.02008 -0.00283 0.00360 0.00091 AFIX 43 H6 2 0.371484 -0.348284 0.024144 11.00000 -1.20000 AFIX 0 C7 1 0.194018 -0.012238 0.060789 11.00000 0.01982 0.01759 = 0.01678 0.00424 0.00440 -0.00304 N1 3 0.521605 0.216931 0.355412 11.00000 0.01887 0.01821 = 0.02298 -0.00207 0.00275 -0.00175 H1N 2 0.482165 0.386904 0.358527 11.00000 -1.20000 H2N 2 0.595986 0.262389 0.364573 11.00000 -1.20000 N2 3 0.677631 -0.166334 0.287470 11.00000 0.01855 0.02732 = 0.02320 0.00129 0.00582 0.00374 H3N 2 0.715721 -0.305943 0.266862 11.00000 -1.20000 H4N 2 0.680561 -0.189505 0.350414 11.00000 -1.20000 O1 4 0.133703 0.197540 0.085857 11.00000 0.02080 0.02149 = 0.02343 0.00130 0.00261 0.00472 O2 4 0.150109 -0.199783 -0.008406 11.00000 0.02275 0.02316 = 0.02152 -0.00168 0.00309 -0.00225 HKLF 4 REM pw0710 in P2(1)/n REM wR2 = 0.0742, GooF = S = 1.048, Restrained GooF = 1.048 for all data REM R1 = 0.0310 for 1105 Fo > 4sig(Fo) and 0.0423 for all 1345 data REM 119 parameters refined using 0 restraints END WGHT 0.0282 0.5088 REM Instructions for potential hydrogen bonds HTAB N1 O1_$3 HTAB N2 N2_$8 HTAB N2 O2_$9 REM Highest difference peak 0.271, deepest hole -0.275, 1-sigma level 0.061 Q1 1 0.5057 -0.0822 0.2564 11.00000 0.05 0.27 Q2 1 0.4140 0.0341 0.2469 11.00000 0.05 0.25 Q3 1 0.2702 0.0112 0.0868 11.00000 0.05 0.25 Q4 1 0.5043 0.1309 0.2935 11.00000 0.05 0.24 Q5 1 0.4677 0.0890 0.3927 11.00000 0.05 0.20 Q6 1 0.7017 -0.0131 0.2548 11.00000 0.05 0.20 Q7 1 0.7145 -0.0493 0.4002 11.00000 0.05 0.19 Q8 1 0.5853 -0.3074 0.0993 11.00000 0.05 0.19 Q9 1 0.4389 0.1454 0.2281 11.00000 0.05 0.18 Q10 1 0.5319 0.0532 0.3812 11.00000 0.05 0.18 ; _shelx_res_checksum 6511 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn1 0.000000 0.500000 0.000000 0.01883(17) Uani d 1 . . C C1 0.32186(18) -0.0488(5) 0.11717(15) 0.0195(5) Uani d 1 . . C C2 0.36414(18) 0.1055(5) 0.20598(15) 0.0198(5) Uani d 1 . . H H2 0.312438 0.241153 0.228031 0.024 Uiso calc 1 . . C C3 0.48037(18) 0.0642(5) 0.26264(15) 0.0192(5) Uani d 1 . . C C4 0.55799(18) -0.1335(5) 0.23063(16) 0.0204(5) Uani d 1 . . C C5 0.51634(19) -0.2802(5) 0.13985(17) 0.0254(5) Uani d 1 . . H H5 0.568982 -0.407707 0.115733 0.030 Uiso calc 1 . . C C6 0.39925(19) -0.2419(5) 0.08470(16) 0.0242(5) Uani d 1 . . H H6 0.371484 -0.348284 0.024144 0.029 Uiso calc 1 . . C C7 0.19402(18) -0.0122(5) 0.06079(14) 0.0181(4) Uani d 1 . . N N1 0.52161(17) 0.2169(4) 0.35541(13) 0.0205(4) Uani d 1 . . H H1N 0.482(2) 0.387(6) 0.3585(18) 0.025 Uiso d 1 . . H H2N 0.596(2) 0.262(6) 0.3646(18) 0.025 Uiso d 1 . . N N2 0.67763(16) -0.1663(5) 0.28747(15) 0.0229(4) Uani d 1 . . H H3N 0.716(2) -0.306(6) 0.2669(18) 0.028 Uiso d 1 . . H H4N 0.681(2) -0.190(6) 0.350(2) 0.028 Uiso d 1 . . O O1 0.13370(12) 0.1975(3) 0.08586(11) 0.0224(4) Uani d 1 . . O O2 0.15011(13) -0.1998(3) -0.00841(11) 0.0229(4) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn1 0.0190(3) 0.0173(3) 0.0187(3) 0.00075(19) 0.00188(18) 0.00021(19) C1 0.0194(10) 0.0188(12) 0.0196(10) -0.0010(8) 0.0034(9) 0.0023(8) C2 0.0198(10) 0.0176(11) 0.0225(11) 0.0022(8) 0.0064(9) 0.0021(9) C3 0.0198(10) 0.0200(12) 0.0171(10) -0.0027(8) 0.0033(8) 0.0013(8) C4 0.0165(10) 0.0203(11) 0.0238(11) -0.0015(9) 0.0041(9) 0.0039(9) C5 0.0233(11) 0.0276(13) 0.0265(12) 0.0059(10) 0.0088(9) -0.0022(10) C6 0.0258(11) 0.0256(12) 0.0201(11) 0.0009(10) 0.0036(9) -0.0028(9) C7 0.0198(10) 0.0176(10) 0.0168(10) -0.0030(9) 0.0044(8) 0.0042(9) N1 0.0189(9) 0.0182(10) 0.0230(9) -0.0018(8) 0.0027(8) -0.0021(8) N2 0.0185(9) 0.0273(11) 0.0232(10) 0.0037(8) 0.0058(8) 0.0013(9) O1 0.0208(8) 0.0215(8) 0.0234(8) 0.0047(6) 0.0026(6) 0.0013(6) O2 0.0227(8) 0.0232(8) 0.0215(8) -0.0022(6) 0.0031(6) -0.0017(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Mn1 O1 . 3_565 180.0 ? O1 Mn1 O2 . 3 93.20(6) ? O1 Mn1 O2 3_565 3 86.80(6) ? O1 Mn1 O2 . 1_565 86.80(6) ? O1 Mn1 O2 3_565 1_565 93.20(6) ? O2 Mn1 O2 3 1_565 180.0 ? O1 Mn1 N1 . 4_565 90.52(6) ? O1 Mn1 N1 3_565 4_565 89.48(6) ? O2 Mn1 N1 3 4_565 93.25(6) ? O2 Mn1 N1 1_565 4_565 86.75(6) ? O1 Mn1 N1 . 2 89.48(6) ? O1 Mn1 N1 3_565 2 90.52(6) ? O2 Mn1 N1 3 2 86.75(6) ? O2 Mn1 N1 1_565 2 93.25(6) ? N1 Mn1 N1 4_565 2 180.0 ? C6 C1 C2 . . 118.93(19) ? C6 C1 C7 . . 121.50(18) ? C2 C1 C7 . . 119.54(19) ? C3 C2 C1 . . 121.0(2) ? C3 C2 H2 . . 119.5 ? C1 C2 H2 . . 119.5 ? C2 C3 C4 . . 120.14(19) ? C2 C3 N1 . . 120.44(19) ? C4 C3 N1 . . 119.41(18) ? C5 C4 C3 . . 118.65(19) ? C5 C4 N2 . . 121.6(2) ? C3 C4 N2 . . 119.64(19) ? C6 C5 C4 . . 120.7(2) ? C6 C5 H5 . . 119.7 ? C4 C5 H5 . . 119.7 ? C5 C6 C1 . . 120.6(2) ? C5 C6 H6 . . 119.7 ? C1 C6 H6 . . 119.7 ? O1 C7 O2 . . 123.23(18) ? O1 C7 C1 . . 118.20(18) ? O2 C7 C1 . . 118.53(19) ? C3 N1 Mn1 . 2_545 120.83(14) ? C3 N1 H1N . . 112.9(16) ? Mn1 N1 H1N 2_545 . 98.0(16) ? C3 N1 H2N . . 109.6(17) ? Mn1 N1 H2N 2_545 . 107.0(17) ? H1N N1 H2N . . 107(2) ? C4 N2 H3N . . 113.5(17) ? C4 N2 H4N . . 111.1(16) ? H3N N2 H4N . . 111(2) ? C7 O1 Mn1 . . 131.83(13) ? C7 O2 Mn1 . 1_545 121.03(13) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 O1 . 2.1591(14) ? Mn1 O1 3_565 2.1591(14) ? Mn1 O2 3 2.2062(15) ? Mn1 O2 1_565 2.2062(15) ? Mn1 N1 4_565 2.3065(19) ? Mn1 N1 2 2.3065(19) ? C1 C6 . 1.391(3) ? C1 C2 . 1.392(3) ? C1 C7 . 1.492(3) ? C2 C3 . 1.384(3) ? C2 H2 . 0.9500 ? C3 C4 . 1.402(3) ? C3 N1 . 1.432(3) ? C4 C5 . 1.397(3) ? C4 N2 . 1.413(3) ? C5 C6 . 1.383(3) ? C5 H5 . 0.9500 ? C6 H6 . 0.9500 ? C7 O1 . 1.261(3) ? C7 O2 . 1.277(3) ? N1 H1N . 0.88(3) ? N1 H2N . 0.86(3) ? N2 H3N . 0.85(3) ? N2 H4N . 0.88(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1N O1 2 0.88(3) 2.19(3) 3.022(3) 156(2) yes N2 H3N N2 2_645 0.85(3) 2.26(3) 3.106(3) 178(2) yes N2 H4N O2 4_656 0.88(3) 2.15(3) 3.008(2) 167(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -1.4(3) ? C7 C1 C2 C3 . . . . 176.57(19) ? C1 C2 C3 C4 . . . . 0.5(3) ? C1 C2 C3 N1 . . . . -178.0(2) ? C2 C3 C4 C5 . . . . 1.6(3) ? N1 C3 C4 C5 . . . . -179.9(2) ? C2 C3 C4 N2 . . . . 177.9(2) ? N1 C3 C4 N2 . . . . -3.5(3) ? C3 C4 C5 C6 . . . . -2.9(3) ? N2 C4 C5 C6 . . . . -179.1(2) ? C4 C5 C6 C1 . . . . 2.0(3) ? C2 C1 C6 C5 . . . . 0.1(3) ? C7 C1 C6 C5 . . . . -177.8(2) ? C6 C1 C7 O1 . . . . -169.7(2) ? C2 C1 C7 O1 . . . . 12.4(3) ? C6 C1 C7 O2 . . . . 12.3(3) ? C2 C1 C7 O2 . . . . -165.55(19) ? C2 C3 N1 Mn1 . . . 2_545 89.4(2) ? C4 C3 N1 Mn1 . . . 2_545 -89.1(2) ? O2 C7 O1 Mn1 . . . . -40.5(3) ? C1 C7 O1 Mn1 . . . . 141.59(15) ? O1 C7 O2 Mn1 . . . 1_545 -60.8(2) ? C1 C7 O2 Mn1 . . . 1_545 117.02(17) ? _cod_database_fobs_code 2243406